反应详情

温度

60 °C

Triethylamine (18 μL, 0.126 mmol) was added to a solution of the bis hydrochloride salt of 2-[(6S,9R)-9-amino-6-(2,3-difluorophenyl)-6,7,8,9-tetrahydro-5H-[1,2,4]triazolo[4,3-a]azepin-3-yl]propan-2-ol (20 mg, 0.051 mmol) and 1,1′-carbonyldiimidazole (14 mg, 0.09 mmol) in tetrahydrofuran (1.0 mL) at 0° C. After 10 min, additional 1,1′-carbonyldiimidazole (8.0 mg, 0.05 mmol) was added. After 30 min, the hydrochloride salt of 2,8-diazaspiro[4.5]decan-1-one (12 mg, 0.06 mmol) and dichloromethane (1.0 mL) were added and the mixture was heated to 60° C. After 16 h, the reaction was concentrated. Purification by reverse phase HPLC (C-18, 10% acetonitrile/water→100% acetonitrile with 0.1% trifluoroacetic acid) gave the title compound (20 mg). MS 503.2570 (M+1).

1. waitAfter 30 min
2. waitAfter 16 h
3. concentrationthe reaction was concentrated
4. customPurification by reverse phase HPLC (C-18, 10% acetonitrile/water→100% acetonitrile with 0.1% trifluoroacetic acid)